ABSTRACT

Introduction .................................................................................................... 136 Materials and methods .................................................................................. 137

Headspace analysis ................................................................................... 138 Automated solid-phase microextraction analysis ................................ 139 Quantitative gas chromatography/selected ion monitoring-mass selective detection analyses ..................................... 140

Sample preparation ........................................................................................ 140 Microwave-scale quantities, sealed vessels ........................................... 140 Pilot-scale quantities, sealed vessels ........................................................141 Open vessels ................................................................................................141 Reagents .......................................................................................................141

Results and discussion ...................................................................................141 Qualitative and relative quantitative analyses, reactions in sealed vessels ........................................................................ 142 Initial quantitative analyses (pyrazine standard) and relative quantitative analyses (cyclohexanone internal standard) ................... 154

Model reactions .............................................................................................. 157 Quantitative gas chromatography/selected ion monitoring-mass selective detection analyses employing multiple authentic pyrazine standards .............................. 166 Open vessel reactions ................................................................................167 Studies employing aqueous solutions and suspensions containing labeled reagents (sealed vessels) ......................................... 170

Summary and conclusions ............................................................................ 179 Acknowledgments ......................................................................................... 179 References ........................................................................................................ 179